1,1,1-Tris(4-hydroxyphenyl)ethane synthesis
- Product Name:1,1,1-Tris(4-hydroxyphenyl)ethane
- CAS Number:27955-94-8
- Molecular formula:C20H18O3
- Molecular Weight:306.36
Yield:27955-94-8 91.3%
Reaction Conditions:
with hydrogenchloride;zinc(II) chloride in water at 60; for 9.66667 h;Reagent/catalyst;
Steps:
1 Example 1
Synthesis method:The reactor was charged with 54.0 moles of phenol and 100 partsGrams of zinc chloride,Stirring to make it mixed evenly,Followed by slow addition over a period of 40 minutes6.5 mol of p-hydroxyacetophenone,After warming up to join Under the conditions of temperature and 60 60 min100 ml of concentrated hydrochloric acid,After the addition, the reaction was stirred for 8 h.After stirring, the temperature was lowered to 20 ° C,Dichloroethane was added,After sufficiently stirring again,filter, 55 vacuum drying 6hThe crude THPE product 1811 grams.The purity of the crude product95.0% and yield 91.1%. Purification method:1000 g of the crude product prepared above was added2000 ml of methanol,Heating completely dissolved,cool down,Slowly add1600 ml of water,Stirred at room temperature for 50 min to give pale yellow product;filter,drying.The dried product was dissolved in 1200 ml of methanol,After complete dissolution by heating,Add activated carbon decolorization, Filtered, the solvent evaporated,The resulting solid;The obtained solid was dissolved in 1000 ml of methanol,A solution of a mixture of sodium borohydride (5 g) and sodium sulfite (35 g) was slowly added,Light yellow powder gradually precipitation,The resulting solid was filtered,Vacuum drying 10 h at 25 ° C to give 913 g of product;The yield was 91.3%HPLC analysis purity 99.5%.
References:
Changzhou Tianhua Pharmaceutical Co., Ltd.;Li, Jianping CN105541561, 2016, A Location in patent:Paragraph 0021; 0022; 0023; 0024; 0025
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80-05-7
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108-95-2
709 suppliers
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27955-94-8
260 suppliers
$5.00/5g
123-54-6
558 suppliers
$10.00/25ml
108-95-2
709 suppliers
$14.00/25g
27955-94-8
260 suppliers
$5.00/5g